Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

5-L-孟氧基4-苄氨基丁烯内酯的不对称合成和晶体结构研究

温和条件下,苄胺与手性合成子5-(L)-孟氧基3-溴-2(5)呋喃酮通过串联的不对称迈克尔加成/分子内消除反应合成了一种新手性化合物:5-L-孟氧基-4-苄胺基丁烯内酯。产物经过IR、1H-NMR、MS谱学表征,并经X-ray单晶衍射测定了其结构。新化合物属于正交晶系,P212121空间群,a=5.2945(4),b=14.2829(10),c=26.0769(18),Mr=343.45,Z=4,V=1972.0(2)3,Dc=1.157g/cm3,μ(MoKα)=0.076mm-1,F(000)=744,R=0.0387,wR=0.0880。     

Synthesis, Crystal Structure and Conformational Analysis of(E)-5-Methoxy-2-((4-methoxyphenylimino)methyl)phenol

The title compound,(E)-5-methoxy-2-((4-methoxyphenylimino)methyl)phenol(C15H15NO3),crystallizes in monoclinic,space group P21/c with a=9.4361(6),b=10.6212(5),c=12.9338(9),β=93.064(5)o,V=1294.41(14)3,Z=4,Dc=1.320 g/cm3,F(000)=544,Rint=0.116,T=296 K,μ=0.09 mm-1,the final R=0.051 and wR=0.148 for 1836 observed reflections with I2σ(I).An extensive two-dimensional network of C-H…O hydrogen bonds and π-ring interactions are responsible for the crystal stabilization.Intermolecular hydrogen bonds and C-H…π interactions produce R22(14),R44(30) and R44(31) rings.In addition to the molecular geometry from X-ray experiment,the molecular geometry of the title compound in the ground state has been calculated using the semi-empirical(AM1 and PM3) and density functional theory method(DFT)(B3LYP) with 6-31G(d) basis set.To determine the conformational flexibility,molecular energy profile of the title compound was obtained by semi-empirical(PM3 and AM1) and DFT/B3LYP calculations with respect to the selected degree of torsional freedom,which varied from -180° to +180° in a step of 10°.     

Hydrothermal Synthesis and Crystal Structure of a Zinc(Ⅱ) Polymer with a Two-dimensional Layer Structure: [Zn(pzdc)(phen)] n·nH_2O

A metal-organic coordination compound formulated as [Zn(pzdc)(phen)] n·nH_2O 1 (H_2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system,space group P2_(1/n) with α=11.607(2),b=11.719(2),c=13.140(3)(A),β=110.707(3)°,V=1671.9(6)(A)~3,C_(18)H_(12)ZnN_4O_5,Mr=429.69,D_c=1.707 g/cm~3,μ(MoKα)=1.511 mm~(-1),F(000)=872,Z=4,the final R=0.0356 and wR=0.0853 for 2713 observed reflections (Ⅰ> 2σ(Ⅰ). It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.     

Synthesis and Crystal Structure Analysis of 2-（3,5-Di-tert-butyl-2-hydroxyphenyl）-2-（3,4- dimethylphenyl） Acetic Acid Dimethylamine Salt

A new compound 2-（3,5-di-tert-butyl-2-hydroxyphenyl）-2-（3,4-dimethylphenyl） acetic acid dimethylamine salt （[NH2（CH3）2][C24H31O3]） was synthesized and structurally determined. It is of monoclinic system, space group P21/c with a = 14.731（2）, b = 10.1185（10）, c = 17.065（2） A^°, β = 98.293（10）° ,Z = 4, V = 2517.0（6）A^°^3, Dc = 1.091 g/cm^3, F（000） = 904 and Mr= 413.58. The dihedral angle defined by two benzene rings is 98.23°.     

A One-dimensional Metallic Oxide Constructed from Molybdenum Clusters and Mn（Ⅱ）-[3-（2-pyridyl） pyrazole] Cationic Coordination Components

A new polyoxomolybdate compound [Mn II (L) 2 (Mo 8 O 26) 0.5 ] 2n (1,L=3-(2-pyridyl)pyrazole) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses,TG and IR spectroscopy.The compound crystallizes in the triclinic system,space group P1 with a=10.063(4),b=11.554(5),c=11.554(5),α=88.89,β=74.839(4),γ=74.839(4)o,V=1249.8(9) 3,C 16 H 14 MnMo 4 N 6 O 13,M r=937.03,D c=2.490 g/cm 3,μ(MoKα)=2.521 mm 1,F(000)=898,Z=2,the final R=0.0390 and wR=0.0970 for 4000 observed reflections (I > 2σ(Ⅰ)).Single-crystal X-ray diffraction analysis results reveal that compound 1 owns a chain structure based on β-[Mo 8 O 26 ] 4anions,which are linked by Mn II (L) 2 units via the terminal oxygen atoms.     

Synthesis, Structural Features and Evaluation of Antibacterial Activities of Two Schiff Bases Derived from 3,4-Dihydroxybenzhydrazide

A new Schiff base compound (I), (E)-N'-(2-hydroxy-3-methoxybenzylidene)-3,4-dihydroxybenzohydrazide-ethanol-water (1/1/1), has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.459(4), b = 18.316(10), c = 13.638(7), β = 101.585(9)o, V = 1825.2(17)3, Z = 4, μ = 0.104 mm-1, Dc = 1.333 g/cm3, F(000) = 776, the final R = 0.0635 and wR = 0.1302 for 3216 observed reflections with I 2σ(I). Another compound (Ⅱ), (E)-N'-(2,5-dimethoxybenzylidene)-3,4-dihydroxybenzohydrazide-ethanol-water (1/1/1), has been synthesized and reported before. The antibacterial activities of these two compounds against seven bacteria were first evaluated, and one compound showed considerable antibacterial activity against S. aureus.     

Synthesis and Crystal Structure of a Heterometallic Chain Coordination Polymer:{[Ni_2Mn_2L_2(CH_3CH_2OH)(H_2O)]·CH_3OH·2H_2O}_n

A chain-like coordination polymer with the chemical formula of {[Ni2Mn2L2(CH3CH2OH)-(H2O)]·CH3OH·2H2O}n has been synthesized by the assembly reaction of K2NiL·H2O and Mn(OAC)2·4H2O with a 1:1 mole ratio in methanol,where OAC-=CH3COO-and H4L=2-hydroxy-3-[(E)-({2-[(2-hydroxybenzoyl)imino]ethyl}imino)methyl]benzoic acid.The crystal structure was determined by single-crystal X-ray diffraction analysis.It belongs to the triclinic system,space group P1,with a=9.9464(8),b=13.4718(11),c=14.3877(12),α=87.1930(10),β=85.4280(10),γ=74.6470(10)°,V=1852.4(3)3,Z=2,Dc=1.807g/cm3,Mr=1008.03,λ(MoKα)=0.71073,μ(MoKα)=1.794 mm-1,F(000)=1032,R=0.0527 and wR=0.1284(Ⅰ2σ(Ⅰ)).The compound exhibits a chain-like structure formed by dissymmetrical tetranuclear units.     

A Stable 'Three-in-one'Coordination Polymer

The title compound[Cu2(IB)2(HIB)2]1 was synthesized via the hydrothermal reaction of CuSO4·5H2O and NaOH with 4-(1H-Imidazol-1-yl)benzoic acid(HIB),and characte-rized by elemental analysis and infrared spectra.The crystal of 1 crystallizes in monoclinic,space group C2/c with a=24.513(8),b=18.948(5),c=17.248(6)(A),β=119.81(2)°,V=6951(4)(A)3,Z=8,C40H30Cu2N8O8,Mr=877.80,Dc=1.678 g/cm3,F(000)=3584 and μ(MoKa)=1.295 mm-1.The final R=0.0542 and wR=0.1335 for 5398 observed reflections with I>2σ(I)and R=0.0845 and wR=0.1520 for all data.X-ray diffraction analysis reveals that the title complex is a unique 'three-in-one'crystal of coordination network through strong hydrogen bonds and coordination covalent bonds.The thermogravimetric analysis measurement showed that compound 1 has thermal stability as no strictly clean weight loss step occurs below 300℃.     

Synthesis and Crystal Structure of (E)2-(3''''-Bromo-5''''-chloro-salicylidene amino)-4-methyl Pyridine

A new Schiff base compound,2-bromo-4-chloro-6-[(4-methylpyridin-2-ylimino)me-thyl]phenol(C13H10BrClN2O),has been synthesized by the condensation of equimolar 3-bromo-5-chlorosalicylaldehyde and 4-methylpyridin-2-ylamine in a methanol solution.The compound Was characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21 with a=6.048(3),b=14.063(7),c=7.623(4)(A),β=97.703(7)°,Z=2,V=642.5(6)(A)3,Dc=1.683 g/cm3,Mr=325.59,λ(MoKa)=0.71073(A),μ=3.395 mm-1,F(000)=324,R=0.0370 and wR=0.0662.A total of 3879 reflections were collected,of which 1970 with,I＞2σ(I)were observed.As expected.the molecule adopts a trans configuration about the C=N double bond.The benzene and pyridine rings are nearly coplanar(mean deviation from the combined plane is 0.031(3)(A)),with their dihedral angle of 3.3(3)°.The preliminary biological tests show that the compound has excellent antibacterial activities.     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

Synthesis and Crystal Structure of (Z)-4-(p-Bromo phenylthio)-3-(p-nitrobenzoyloxy)-3-buten-2-one

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｏｒｄｅｒｔｏｅｖａｌｕａｔｅｔｈｅｓｅｌｅｃｔｉｖｉｔｙａｎｄｒｅａｃｔｉｖｉｔｙｏｆｅｎｏｎｅｓａｓｄｉｅｎｏｎｅｐｈｉｌｅｓａｎｄｄｉｅｎｅｓｉｎＤｉｅｌｓＡｌｄｅｒｒｅａｃｔｉｏｎ,Ｐａｒａｌｔａｓｙｎｔｈｅｓｉｚｅｄβｆｕｎｃｔｉｏｎａｌｉｚｅｄｌａｃｅｔｙｌｖｉｎｙｌａｒｅｎｅｃａｒｂｏｘｙｌａｔｅｓａｓａｓｕｂｓｔｒａｔｅｏｆ１,３ｄｉｐｏｌａｒｃｙｃｌｏａｄｄｉｏｎｒｅａｃｔｉｏｎ〔１〕．Ｘｒａｙｃｒｙｓｔａｌｌｏｇｒａｐｈｉｃｓｔｕｄ…     

Cationic diiron and diruthenium μ-allenyl complexes: synthesis, X-ray structures and cyclization reactions with ethyldiazoacetate/amine affording unprecedented butenolide- and furaniminium-substituted bridging carbene ligands

The novel cationic diiron μ-allenyl complexes [Fe(2)Cp(2)(CO)(2)(μ-CO){μ-η(1):η(2)(α,β)-C(α)(H)=C(β)=C(γ)(R)(2)}](+) (R = Me, 4a; R = Ph, 4b) have been obtained in good yields by a two-step reaction starting from [Fe(2)Cp(2)(CO)(4)]. The solid state structures of [4a][CF(3)SO(3)] and of the diruthenium analogues [Ru(2)Cp(2)(CO)(2)(μ-CO){μ-η(1):η(2)(α,β)-C(α)(H)=C(β)=C(γ)(R)(2)}][BPh(4)] (R = Me, [2a][BPh(4)]; R = Ph, [2c][BPh(4)]) have been ascertained by X-ray diffraction studies. The reactions of 2c and 4a with Br?nsted bases result in formation of the μ-allenylidene compound [Ru(2)Cp(2)(CO)(2)(μ-CO){μ-η(1):η(1)-C(α)=C(β)=C(γ)(Ph)(2)}] (5) and of the dimetallacyclopentenone [Fe(2)Cp(2)(CO)(μ-CO){μ-η(1):η(3)-C(α)(H)=C(β)(C(γ)(Me)CH(2))C(=O)}] (6), respectively. The nitrile adducts [Ru(2)Cp(2)(CO)(NCMe)(μ-CO){μ-η(1):η(2)-C(α)(H)=C(β)=C(γ)(R)(2)}](+) (R = Me, 7a; R = Ph, 7b), prepared by treatment of 2a,c with MeCN/Me(3)NO, react with N(2)CHCO(2)Et/NEt(3) at room temperature, affording the butenolide-substituted carbene complexes [Ru(2)Cp(2)(CO)(μ-CO){μ-η(1):η(3)-C(α)(H)[upper bond 1 start]C(β)C(γ)(R)(2)OC(=O)C[upper bond 1 end](H)] (R = Me, 10a; R = Ph, 10b). The intermediate cationic compound [Ru(2)Cp(2)(CO)(μ-CO){μ-η(1):η(3)-C(α)(H)[upper bond 1 start]C(β)C(γ)(Me)(2)OC(OEt)C[upper bond 1 end](H)](+) (9) has been detected in the course of the reaction leading to 10a. The addition of N(2)CHCO(2)Et/NHEt(2) to 7a gives the 2-furaniminium-carbene [Ru(2)Cp(2)(CO)(μ-CO){μ-η(1):η(3)-C(α)(H)[upper bond 1 start]C(β)C(γ)(Me)(2)OC(OEt)C[upper bond 1 end](H)](+) (11). The X-ray structures of 10a, 10b and [11][BF(4)] have been determined. The reactions of 4a,b with MeCN/Me(3)NO result in prevalent decomposition to mononuclear iron species.     

Syntheses and Structures of Two Novel Salicylate-containing Mononuclear Manganese Complexes

Two salicylate containing mononuclear manganese complexes formulated as [Mn- (sal)2(CH3OH)2]·py (sal = salicylate, py = pyridine) 1 and (HNEt3)2[Mn(sal)3] 2 have been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction analyses. Crystal data for compound 1: monoclinic, space group C2/c, a = 30.748(6), b = 8.1933(13), c = 21.137(4) °, β = 126.772(4)°, V = 4265.5(13) 3, Z = 8, Mr = 471.34, Dc = 1.468 g/cm3, μ = 0.667 mm-1, F(000) = 1952, the final R = 0.0637, wR = 0.1783 (I > 2σ(I)) and GOOF = 1.073; and those for compound 2: monoclinic, space group C2/c, a = 14.505(5), b = 11.048(4), c = 20.711(7) , β = 103.603(6)°, V = 3225.6 (18) 3, Z = 4, Mr = 668.65, Dc = 1.377 g/cm3, μ = 0.466 mm-1, F(000) = 1416, the final R = 0.0373, wR = 0.1125 (I > 2σ(I)), and GOOF = 1.000. The Mn atoms of both complexes are six-coordinated in an axially elongated octahedral geometry for 1 and an axially compressed octahedral geometry for 2, and their oxidation states have been determined to be trivalent by bond valence sum calculation.     

Synthesis, Crystal Structure and Antitumor Activity of （E）-4-tert-Butyl-N-（2,4-dichlorobenzylidene）-5-（1,2,4-triazol-1-yl）-thiazol-2-amine

The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobenzaldehyde, and its crystal structure was determined by singlecrystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9748(4), b = 10.1803(5), c = 11.4603(6), α = 102.882(1), β = 100.253(1), γ = 104.457(1)°, V = 850.95(7)3, Z = 2, F(000) = 392, C16H15Cl2N5S, Mr = 380.29, Dc = 1.484 g/cm3, S = 1.095, μ = 0.512 mm-1, the final R = 0.0301 and wR = 0.0965 for 3334 observed reflections (I 2σ(I)). The preliminary antitumor activity shows that for the title compound the IC50 of Hela is 0.175 μmol/mL and that of Bel7402 is 0.156 μmol/mL.     

5-芳基-3-二茂铁基二氢吡唑的合成及晶体结构

吡唑环是许多具有生理活性化合物的关键结构,许多吡唑衍生物都显示了较强的生理活性,如镇静止痛、消炎、杀菌、降血糖以及安眠的活性等~([1-3]),特别是芳基吡唑在医药以及农药方面具有重要的应用~([4,5]).     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Coordination Polymer Constructed from Bicapped Pseudo-Keggin Cluster:(Et_3N)_(0.5)(en)_2[SiMo_(12)O_(40)(VO)_2]·4H_2O

A new pseudo Keggin-type bicapped compound(Et3N)0.5(en)2[SiMo12O40(VO)2]·4H2O(Et3N=triethylamine,en=ethylenediamine) has been hydrothermally synthesized and characterized by IR,elemental analysis,TG and X-ray crystallography.The title compound crystallizes in monoclinic,space group P21/n with a=17.576(2),b=13.535(1),c=21.587(2),β=103.790(10)°,V=4987.3(8)3,Z=4,Dc=2.925 Mg/m3,Mr=2196.12,F(000)=4148,μ=3.400 mm-1,R=0.0379 and wR=0.1219.The most remarkable structural feature of the compound is that the clusters represent bicapped pseudo-Keggin structure and are linked one by one through V-O-V bonds forming an infinite 1D chain.Furthermore,such chains are interconnected in a cross-like arrangement through multiform hydrogen bonds to yield a 3D supramolecular network.     

Synthesis,Crystal Structure and Antimicrobial Property of 4-Bromo-2-[(3-methypyridin-2-ylimino)methyl]phenol

The title Schiff base compound 4-bromo-2-[(3-methylpyridin-2-ylimino)me-thyl]phenol was prepared and structurally characterized by elemental analysis,IR spectrum,and single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n,with a=4.4870(9),b=19.953(4),c=13.860(3)(A),β=93.13(3)°,V=1239.O(4)(A)3,Z=4,Dc=1.561g/cm3,C13H11BrN2O2,Mr=291.15,μ=3.302mm-1 and F(000)=584.The final refinement gave R =0.0608 and wR=0.1377 for 1329 observed reflections with I＞2σ(I).X-ray diffraction reveals that the non-hydrogen atoms in the compound are nearly coplanar,with the mean deviation of 0.0197 (A) from the plane.The molecule adopts an E configuration about the central C=N functional bond.The compound possesses moderate antimicrobial property.     

Asymmetric Synthesis and Crystal Structure of （-）-N-[（3R）-3-Cyclohexyl]-3-phenylpropananoyl]bornane-10,2-sultam

The title compound (-)-N-[(3R)-3-cyclohexyl]-3-phenylpropananoyl]bornane-10,2sultam (C 25 H 35 NO 3 S,M r=429.60),a derivative of camphorsultam,crystallizes in the monoclinic space group P2 1 /c with a=10.3301(7),b=19.4040(13),c=11.8106(8),β=100.5580(10)°,V=2327.3(3) 3,Z=4,D c=1.226 g/cm 3,λ=0.71073,μ(MoKα)=0.165 mm-1 and F(000)=928.X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat form (Fig.1).The planes constructed by (C(4),C(5),C(6),C(7)) and (C(7),C(8),C(9),C(4)) form a dihedral angle of 69.5°.The C(1)-C(2)-C(3) plane forms dihedral angles to the aforementioned planes of 89.8(1) and 85.9(3)°,respectively.And molecules are linked via hydrogen bonding (C-H···N/O) interactions.     

Synthesis and Crystal Structur of (4,4''-H2bipy)[CdBr4]·H2O

The title compound (4,4'-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoelinic,space group P21/c with a=8.260(3), b=23.926(7), c=9.774(2) (A), β=106.777(9)°,C10H12Br4CdN2O, Mr=608.26, V=1849.4(9)(A)3, Z=4, Dc=2.185 g/cm3, S=1.005, μ(MoKα)=9.814 mm-1, F(000)=1128, R=0.0646 and wR=0.0989. The crystal structure analysis of 1reveals that the title compound features an isolated structure, based on discrete 4,4'-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetrahedral cadmium atoms terminally coordinated by four bromine atoms.